#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/91/4109136.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4109136
loop_
_publ_author_name
'Yuichi Shimazaki'
'Tatsuo Yajima'
'Fumito Tani'
'Satoru Karasawa'
'Koichi Fukui'
'Yoshinori Naruta'
'Osamu Yamauchi'
_publ_section_title
;
 Syntheses and Electronic Structures of One-Electron-Oxidized Group 10
 Metal(II)-(Disalicylidene)diamine Complexes (Metal = Ni, Pd, Pt)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2559
_journal_page_last               2568
_journal_paper_doi               10.1021/ja067022r
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C32 H46 N2 Ni O2 '
_chemical_formula_sum            'C32 H46 N2 Ni O2'
_chemical_formula_weight         549.43
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.287(6)
_cell_length_b                   10.919(3)
_cell_length_c                   10.265(3)
_cell_measurement_reflns_used    23106
_cell_measurement_temperature    133.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     2946.3(14)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9985
_diffrn_measured_fraction_theta_max 0.9985
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7656
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3380
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.0077
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.01000(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                1745
_reflns_number_total             3380
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja067022rsi20060930_040118.cif
_cod_data_source_block           SHIMAZAKI
_cod_original_cell_volume        2946(1)
_cod_original_formula_sum        'C32 H46 N2 Ni O2 '
_cod_database_code               4109136
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2-y,1/2+z
1/2+x,1/2-y,-z
-x,y,1/2-z
-x,-y,-z
1/2+x,1/2+y,1/2-z
1/2-x,1/2+y,z
x,-y,1/2+z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ni(1) Ni 0.5000 0.02409(4) 0.7500 0.0142(1) Uani 1.00 d S
O(1) O 0.53425(7) 0.1474(2) 0.8362(2) 0.0174(5) Uani 1.00 d .
N(1) N 0.52685(9) -0.0995(2) 0.8517(2) 0.0169(7) Uani 1.00 d .
C(1) C 0.5731(1) 0.1352(3) 0.9156(3) 0.0160(7) Uani 1.00 d .
C(2) C 0.60531(10) 0.2385(3) 0.9411(3) 0.0165(7) Uani 1.00 d .
C(3) C 0.64391(10) 0.2238(3) 1.0326(3) 0.0180(8) Uani 1.00 d .
C(4) C 0.65416(10) 0.1148(3) 1.1000(3) 0.0180(7) Uani 1.00 d .
C(5) C 0.62413(9) 0.0161(3) 1.0726(3) 0.0180(7) Uani 1.00 d .
C(6) C 0.58453(9) 0.0232(3) 0.9792(3) 0.0163(8) Uani 1.00 d .
C(7) C 0.5589(1) -0.0879(3) 0.9457(3) 0.0178(8) Uani 1.00 d .
C(8) C 0.5044(1) -0.2198(2) 0.8236(3) 0.0177(7) Uani 1.00 d .
C(9) C 0.5972(1) 0.3594(3) 0.8694(3) 0.0174(8) Uani 1.00 d .
C(10) C 0.5450(1) 0.4146(3) 0.9059(3) 0.0248(9) Uani 1.00 d .
C(11) C 0.5989(1) 0.3378(3) 0.7207(3) 0.0229(9) Uani 1.00 d .
C(12) C 0.6384(1) 0.4543(3) 0.9007(3) 0.0267(9) Uani 1.00 d .
C(13) C 0.6991(1) 0.1092(3) 1.1941(3) 0.0228(8) Uani 1.00 d .
C(14) C 0.70485(10) -0.0178(3) 1.2559(4) 0.0304(8) Uani 1.00 d .
C(15) C 0.6920(1) 0.2027(3) 1.3041(3) 0.0345(10) Uani 1.00 d .
C(16) C 0.7486(1) 0.1382(3) 1.1192(3) 0.0333(9) Uani 1.00 d .
H(1) H 0.6648 0.2948 1.0509 0.0247 Uiso 1.00 calc .
H(2) H 0.6299 -0.0604 1.1174 0.0230 Uiso 1.00 calc .
H(3) H 0.5661 -0.1592 0.9973 0.0223 Uiso 1.00 calc .
H(4) H 0.5264 -0.2851 0.8515 0.0252 Uiso 1.00 calc .
H(5) H 0.4690 -0.2290 0.8709 0.0252 Uiso 1.00 calc .
H(6) H 0.5436 0.4326 0.9970 0.0326 Uiso 1.00 calc .
H(7) H 0.5388 0.4882 0.8585 0.0326 Uiso 1.00 calc .
H(8) H 0.5182 0.3577 0.8864 0.0326 Uiso 1.00 calc .
H(9) H 0.5738 0.2787 0.6968 0.0292 Uiso 1.00 calc .
H(10) H 0.5922 0.4122 0.6760 0.0292 Uiso 1.00 calc .
H(11) H 0.6315 0.3079 0.6960 0.0292 Uiso 1.00 calc .
H(12) H 0.6707 0.4259 0.8777 0.0342 Uiso 1.00 calc .
H(13) H 0.6311 0.5295 0.8572 0.0342 Uiso 1.00 calc .
H(14) H 0.6379 0.4709 0.9938 0.0342 Uiso 1.00 calc .
H(15) H 0.6750 -0.0397 1.3025 0.0376 Uiso 1.00 calc .
H(16) H 0.7108 -0.0788 1.1899 0.0376 Uiso 1.00 calc .
H(17) H 0.7332 -0.0193 1.3145 0.0376 Uiso 1.00 calc .
H(18) H 0.7199 0.2010 1.3630 0.0424 Uiso 1.00 calc .
H(19) H 0.6901 0.2843 1.2672 0.0424 Uiso 1.00 calc .
H(20) H 0.6614 0.1879 1.3503 0.0424 Uiso 1.00 calc .
H(21) H 0.7771 0.1378 1.1766 0.0418 Uiso 1.00 calc .
H(22) H 0.7543 0.0786 1.0522 0.0418 Uiso 1.00 calc .
H(23) H 0.7461 0.2169 1.0794 0.0418 Uiso 1.00 calc .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ni Ni 0.339 1.112
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Ni(1) O(1) 86.3(1) . 4_656 yes
O(1) Ni(1) N(1) 94.36(9) . . yes
O(1) Ni(1) N(1) 172.2(1) . 4_656 yes
O(1) Ni(1) N(1) 172.2(1) 4_656 . yes
O(1) Ni(1) N(1) 94.36(9) 4_656 4_656 yes
N(1) Ni(1) N(1) 86.1(2) . 4_656 yes
Ni(1) O(1) C(1) 127.0(2) . . yes
Ni(1) N(1) C(7) 127.0(2) . . yes
Ni(1) N(1) C(8) 112.9(2) . . yes
C(7) N(1) C(8) 119.9(3) . . yes
O(1) C(1) C(2) 119.5(3) . . yes
O(1) C(1) C(6) 122.6(2) . . yes
C(2) C(1) C(6) 118.0(3) . . yes
C(1) C(2) C(3) 117.6(3) . . yes
C(1) C(2) C(9) 120.7(2) . . yes
C(3) C(2) C(9) 121.8(3) . . yes
C(2) C(3) C(4) 124.8(3) . . yes
C(3) C(4) C(5) 117.2(3) . . yes
C(3) C(4) C(13) 119.7(3) . . yes
C(5) C(4) C(13) 123.1(3) . . yes
C(4) C(5) C(6) 121.5(3) . . yes
C(1) C(6) C(5) 120.9(3) . . yes
C(1) C(6) C(7) 121.4(2) . . yes
C(5) C(6) C(7) 117.6(3) . . yes
N(1) C(7) C(6) 125.0(3) . . yes
N(1) C(8) C(8) 104.8(2) . 4_656 yes
C(2) C(9) C(10) 110.1(2) . . yes
C(2) C(9) C(11) 109.9(2) . . yes
C(2) C(9) C(12) 112.7(2) . . yes
C(10) C(9) C(11) 108.9(3) . . yes
C(10) C(9) C(12) 108.2(2) . . yes
C(11) C(9) C(12) 106.9(3) . . yes
C(4) C(13) C(14) 112.0(2) . . yes
C(4) C(13) C(15) 110.2(2) . . yes
C(4) C(13) C(16) 109.2(2) . . yes
C(14) C(13) C(15) 108.1(3) . . yes
C(14) C(13) C(16) 108.0(2) . . yes
C(15) C(13) C(16) 109.3(3) . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni(1) O(1) 1.846(2) . yes
Ni(1) O(1) 1.846(2) 4_656 yes
Ni(1) N(1) 1.846(2) . yes
Ni(1) N(1) 1.846(2) 4_656 yes
O(1) C(1) 1.313(3) . yes
N(1) C(7) 1.286(4) . yes
N(1) C(8) 1.469(3) . yes
C(1) C(2) 1.435(4) . yes
C(1) C(6) 1.419(4) . yes
C(2) C(3) 1.392(4) . yes
C(2) C(9) 1.526(4) . yes
C(3) C(4) 1.403(4) . yes
C(4) C(5) 1.365(4) . yes
C(4) C(13) 1.527(4) . yes
C(5) C(6) 1.417(4) . yes
C(6) C(7) 1.430(4) . yes
C(8) C(8) 1.528(6) 4_656 yes
C(9) C(10) 1.546(4) . yes
C(9) C(11) 1.545(4) . yes
C(9) C(12) 1.532(4) . yes
C(13) C(14) 1.532(5) . yes
C(13) C(15) 1.534(4) . yes
C(13) C(16) 1.544(4) . yes
